関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Benzoyl chloride | HCID 7412 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-[3-(Imidazol-1-yl)propylamino]-2-methyl-1-propanol | HCID 18349765 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 2-[3-(Imidazol-1-yl)propylamino]2,2-dimethylethyl benzoate dihydrochloride | HCID 18349717 | — |
反応手順
A solution of benzoyl chloride (0.36 g) in dichloromethane (1.5 ml) was added dropwise to a mixture of 2-[3-(imidazol-1-yl)propylamino]-2-methyl-1-propanol (0.5 g) and triethylamine (0.5 g) in dichloromethane (5 ml) with stirring under nitrogen at 0° C. The mixture was stirred at 0° C. for 1 hour and then allowed to warm up to ambient temperature and stirred at this temperature for 3 hours. Saturated aqueous sodium bicarbonate (5 ml) was added. The mixture was shaken and the organic layer separated. The aqueous layer was extracted with further dichloromethane. The combined organic extracts were dried, filtered and evaporated to give an oil which was dissolved in ether and treated with ethereal hydrogen chloride to give 2-[3-(imidazol-1-yl)propylamino]-2,2-dimethylethyl benzoate dihydrochloride, m.p. 198-199° C., after recrystallisation from ethanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06215001B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-3d51b09e709441be9219da2c42af2f96 |
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| 出典メモ | uspto-grants-2001_04 |
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